Apparatus for producing and separating certain substances



"Se t. 2 1924.

1506,873 v v. M. WEAVER APPARATUS FOR PRODUCING AND SEPARATING CERTAINSUBSTAN CES Original Filed July 6, 1915 3 hcots-$hoot l lnveruiorflflfor M Weaver Bygf 'l Sept. 2. 1924. V 7 1,506,873-

, V. M. WEAVER APPARATUS FOR PRODUCING AND SEPARATING CERTAIN SUBSTANCESOriginal Filed July e, 1915 s sheds-shut 2 l 72/ 77 g) 77 7a fnaen 230275a for" 157. T VEQJ QW Septr2. 1924. I 1,506.873

V. M. WEAVER A APPARATUS FOR PRODUCING ANIS SBPARATING CERTAINSUBSTANCES Original Filed July 6, 1915 Sheets-Shoot 5 Patented Sept. 2,1924,

v v UNITED STATES vroron M. WEAVER, OF Haas-Issues, rnnnsrtvanrn,assrenos mo EAVER COM:

. PANY, A CORPORATION or "WISCONSIN. 1 Y

arranarus FOB rno nccrne AND sE'ranarInscnnram sues'ranons.

Original application filed. January 7, 1915, Serial No. 919. Divided andthis a pnc auon'siea.nu 'c,

1915, Serial No. 38,386. Renewed November 21, 1919. Serial No. 359,680.

To all whom it may concern.

Be it known that I, VICTOR 11. eaves, a citizen of the United States,residing at Han risburg, in the county of Dauphin and StateotPennsylvania, haveinvented a certain new and useful Improvement inApparatus for Producing and Separating. Certain Sub stances, oi whichthe following is a full, clear, concise, and exact description,reference being had to-the accompanying drawings,- torming a partof thisspecification.

My intention relates to apparatus for carrying out processes of forming,treating and separating chemical compounds or elements depending uponcertain chemical orphysical characteristics, orboth.

The apparatus oimy invention means 1. For the separation or two or moresub stances which condense at different temperatures.

2. For the production of deliquescent substances.

3. For the treatment of substances under the influence of heat, and i 1a. More specifically, for the productio and separation of aluminumchloride and silicon tetrachloride.

It will be clear to those skilled in the art that my invention willadmit oi broader application than the specific uses whichl shalldescribe as an instance of its employment. In order to simplify thisdescription I shall describe my apparatus as employed in carr ing out aprocess of securing aluminum chloride and silicon tetrachloride fromclay and proper reagents and separating these two chlorides. break upthe compound in thepresence of carbon'by the use of chlorine gas so asto produce aluminum chloride, silicon tetrachloride and carbon monoxideand then subject the chlorides which I thus form to conprovides densingtemperatures whereby the two chlorides areseparated and independentlycollected.

This application is division of my copending application, Serial No.91-9, filedJa'nu- 858,001, filed August 22, 1914;, which resulted In thetreatment of clay I in my Patent No. 1,238,60, dated 28,

Myinvention will be more readily. understood by "reference to theaccompanying drawings, in which, 4 I Figure 1' is .a more or lessdiagrammatic representation of the system of apparatus; Figure Q-is'ayertical'secti'onal Viewotthe chloridizi'ng furnace; V

Figure 3 is a horizontal sectional view ot the chloridizingfurnace takenon the plane of the line of Figure '2 andlooking in the directionindicated by the arrows.

Referring first to Figure 1, it will be seen that the chloridizingturnace 1s shown at. 9,

and by reference to Figures 2 and 3 it will be seen that thischloridizing furnace is of the sealed type and provides for a bed ofcoke 10, in which a plurality ot'electrodes 1111, extendinginwardlythrough the circular housing, as illustrated in Figure 3, are lodged.Each ot the carbon electrodes 11 is firmly anounted in a terra cottapipe 12, which inturn is'mounted in the fire brick housing 13. Anelectric conductor 1a is pro vided for each ofthe carboneleetrodes andthis conductor is in the form of a pipe which is connected'with theelectrode at 15 and which is supported in positionby means of a union 16packed at 11'. kept cool by a flow of water introduced through the entrypipe-18, and, after circu illustrated, and at'thi's distance from theturnace housing the conductor and its insulation will not beinpiriously'at'tected by the heat.

The pipe 14E is' The reference character filindicates a cleanout doorwhich may bepr ovide'd, and apeephole arrangemeu p v The chargeintroduced into the chloridizing furnace by way of a'serew conveyor,indicated at at the bottom of a hopper bin 2%, this screw conveyorleading the charge to the passage 25, through which the charge may dropon to the bed-ct COK8 W l11C l1 has already been referred to. The chargeis indicated at 26 and the bed is preferably so arranged thatthe cokeexposed in the middle is surrounded by packed clay, as illustrated at9727. 'The charge may also'be provided. 1

may be any clay, but I have found that the higher grades of clay, suchas kaolin, of the formula Al (SiO (the moisture being driven therefrom)is especially desirable. It will be noted that the furnace has only theoutlet 28 and it will be noted as this description proceeds that theentire system is sealed as this furnace is. It will be noted that agraphite pipe 29 extends through the fire brick housing of the furnaceand term]- nates in the heart of the coke bed. This pipe 29 is fedthrough a pipe 30 (Figure 1) from a storage reservoir 31, the connectionbeing controlled by a valve '32. It will now be noted that, with thechlorine properly fed to the graphite pipe and with the current properlyapplied to the electrodes, the activity of the chlorine gas and the heat1mmediately effects the disintegration of the kaolin, the formation ofaluminum chloride and silicon tetrachloride, and, by the combination ofthe carbon and the oxygen liberated from the kaolin, the formation ofcarbon monoxide.

The reaction is as follows:

The three gases thus formed naturally rise and pass out of the outletopening 28, and, as illustrated in Figure 1, are conducted to thecondenser 33. This condenser is in the form of a double closed chamberproviding the compartment 34 and the co1npart ment 35 separated by apartition 36. The compartment 84 is provided with a system of coolingpipes 3737, which extend downwardly through and from the top of thechamber and which are distributed throughout the entire space of thisparticular compartment in order to get complete temperature control. Thepipes 8737 are joined at the upper ends outside of the chamber by meansof the header ipe 38, and circulation is secured in any desirablemanner. In this particular condenser element the system of pipes isconnected to a cold water supply and the result is that as the threegases which have been referred to enter and pass through the compartment34 the aluminum chloride gas, which condenses at a higher temperaturethan the silicon tetrachloride gas,is condensed and deposits itself as awhite powder upon the pipes 3737. It might be mentioned here that it ispossible that in the action in the chloridizing furnace some otherchloride of silicon might incidentally be formed, a chloride such ashexachloride (Si Cl but I find that conditions are such that it is onlythe silicon tetrachloride which plays any considerable part.

Since the temperature which is produced by the circulation of mere coldwater in the cooling pipes 3737 is not sufficiently low to condensesilicon tetrachloride, this gas, to-

gether with the carbon monoxide, passes on to the next compartment 35 ofthe condenser. Thus the first condenser element 84 is devoted to thecondensation of the aluminum chloride and the white powder to which itis reduced is removed from the pipes upon which it is deposited by meansof the scrapers 39, 39, which, by means of pulley cords 40 passing oversuitable pulleys 41, 41 on the outside of the condenser, are drawn upand down on the pipes to-scrape them, in an obvious manner. The powderis thus thrown down on to the conveyor 42, the upper run a of whichpasses in the direction of the arrow, 43, and thus the condensedaluminum chloride is brought to the end of the condenser element wherethe outlet 44 leading to a tank 45 is provided. This outlet may becontrolled by a valve 46. It will be noted that this tank is connectedby means of a pipe with a compressed air tank 48, which is fed throughthe air compressor 49. It is important, as before indicated, that thesystem be a closed system and that various actions be carried on underpressure, and I speak of it particularly at this time because of thefact that the aluminum chloride to which I have just referred isextremely deliquescent and must be kept free from moisture in. order toavoid decomposition and the formation of hydrochloric acid. When thesystem is closed, however, such aresult is not possible, and thepressure is effective in condensing and keeping condensed this volatilesubstance.

Leaving the aluminum chloride, which has been deposited in the tank 45,for the present, I shall follow the course of the silicon tetrachloridegas and the carbon monoxide through the second element of the condenser.

The condenser element 35 is provided with therefore considerably lowerthan the tem perature in the condenser element 34. The lower temperatureis sufficient to condense the silicon tetrachloride which comes down asa colorless liquid, except for any impurities which may discolor it.This liquid silicon tetrachloride passes down the sloping bottom of thecondenser element 35 and passes through the outlet 55 to a tank 57. Thisoutlet may be controlled by a valve 56. The condenser element 35 isprovided with scrapers. as the condenser element 34 is, be cause it ispossible that aluminum chloride not entirely condensed in its passagethrough the condenser element 34 may condense upon I the time that thesystem is being-worked.

The condenser element 35 is a conveyor 58. r

The'carbon monoxide passes out of the provided with condenser element 35through a pipe 59, past a valve 60 and to a closed gas pump 61-, and isthen carried to a scrubber 62 by means of a pipe 63, this scrubber beingin the form of a tank containing lime water and having an outlet pipe 63leading therefrom. This outlet pipe is provided with a valve 64 andleads to a telescoping gas receiver 65 so that pressure may be kept uponthe carbon monoxide which finds its Way tothis receiver and so that thecarbon monoxide may be fed by way of a pipe 66 to a burner 67, which isused for heating the tank 45 for a purpose to which I shall now refer.

Where additional chlorides are formed in the chloridizing furnace, whichcondense at other temperatures, asis the case when iron or titanium arepresent in the clay, or other ore used, the condenser may be [ar rangedto separate these from the aluminum and silicon chlorides, and from-eachother, by increasing the number of elements maintained at the differenttemperatureswhich are required to separately deposit the: substances. V

Returning now to the aluminum chloride deposited in the form of a powderin the tank 45 (this powder being white unless discolored byimpurities), it will he noted that I have placed the burner 67 underthis tank, and I may mention here that I surround the tank in practicewith a suitable fire wall, so that I can subject thetank to a highdegree of heat. With the valve 46 closed, the material in the tank 45can be placed under high pressure from the tank '48, and this pressuretogether with the heat from-the carbon monoxide burner melts thealuminum chloride, after which step the aluminum chloride is much morestable and much more easily handled, due to its physical condition. Idesire to state, however, that it is entirely feasible to care for thealuminum chloride in its powder condition. r

A pipe '70 leads from the tank 45 to a valve 71, which in turnisconnected with a pipe 72 leading into a furnacefpreferably of theRodenhauser three-phase type. This furnace comprises a heavy outerhousing, which is provided with around bottom 74 mounted in acorrespondingly shaped base 75, the idea being that whenthe connectingpipes are temporarily detached thefurna-ce can be-tilted in order-to;tap 01f molten metal, as will be pointed out alittle later. The liningof the furnace provides a cavity for the molten metal. It willbe seenthat-when the valve 71 is openedthe liquid aluminum chloride isconducted to the working ;cham-; ber of the Rodenhauser furnace.- Theson for this step in the process is as follows:

In the first condensation of the aluminum chloride in the condenserelement 34 there are likely- ;to be impurities, principally ironchloride, unless more than two condenser elements are provided atappropriately different'tem aeratures, .and it is the object of the Jstep inthe process now under description to eliminate this iron and tosecure pure alumi-' num fchloride. Therefore, preliminarily, theRodenhauser furnace is charged with alumis num and the molten bath, asillustrated, is formed, when, as before stated, the .valve '71 is openedand the liquid aluminum chloride is fed into this bath of moltenaluminum near thebottom thereof, the aluminum chlo-. ride is immediatelyreconverted into a gas. due to the. release of pressure and heat of bathand passes up through the molten.v

aluminum. ,Due tothe greaterafi inity vof the chlorine for the aluminumthan for the" iron, or other impurity for that matter, the chlorinereleases the iron and takes on the proper share of aluminum.Theresult-is that the refined aluminum chloride will leave the way valvemaybe provided so that ifdesired the purified aluminum chloride may beled to a separatecondenser, soathat the first condenser: may operatecontinuously and" without the introduction of purified aluminumchloride'ga's. vIt will also appearthat if some of the silicontetrachloride should happen to become condensed in the alumi-, numchloride part of the condenser; system, such condensedsilicontetrachloride'will be removed with the impurities inthe-Rodenhauser furnace since the aluminum has greater affinity forchlorine than silicon and the chlorine will release the silicon and takeup the proportionate share of aluminum, leaving the silicon toimpurities.

It will be seen that the system is a closed systemand that moisture iseffectively ex, cluded so as to protectthe active chlorides,particularly the alumimimlchlorides;''

It will appear-that changes and modifican tions in the apparatus of myinvention will be possible withontdeparting from the spirit and scope ofmy invention and that parts ofthe apparatus may be advantageously em.-'

ployed without employing the other parts 1 be tapped off with the to beunderstood that I contemplate any use to which my apparatus and theindividual parts thereof may be put. I desire, therefore, that theimetesand bounds of my invention shall be determined by the appended claimswhich I have drawn variously so as to bring out the combinations which,of themselves and regardless of their use, are new.

I claim: a V

1. In combination, a sealed furnace, asealed condenser connectedtherewith and having a manually'controlled outlet at the bottom and avalved outlet at the "top, and a sealed tank having sealed connectionwith said manually controlled outlet.

2. In combination, a sealed furnace, a sealed condenser connectedtherewith, sealed gas receiver having sealed connection with saidcondenser, a sealed tank connected with said condenser, and means forheating said tank.

3. In combination, a sealed furnace, a gas storage reservoir havingsealed connection for feeding to said furnace, said furnace having aninlet adapted-to be sealed by the material fed thereto, and a sealedcondenser connected with said furnace, said condenser having a valvedoutlet.

4. In combination, a sealed furnace, a gas storage reservoir havingsealed connection with said furnace, said furnace having an inletadapted to be sealed by the material fed thereto, and a sealed condenserfed from said furnace, said condenser having an outlet to a pump.

5. In combination, a sealed furnace, a gas storage reservoir havingsealed connection with said furnace, said furnace having an inletadapted to be sealed by the material fed thereto, a sealed condenserconnected with said furnace, said condenser having a connection to apump, and a sealed receiver connected with said condenser.

6. In combination, a sealed furnace, a storage reservoir having sealedconnection with said furnace, said furnace having an inlet adapted to besealed by the material fed thereto, a sealed condenser connected withsaid furnace, said condenser having an outlet pipe leading to a pump, asealed tank connected with said condenser, a scrubber to which said pumpdelivers, a gas receiver communicating with said scrubber, said.receiver supplying a pressure feed to a burner, said burner beingdisposed in proximity to said tank.

7. Apparatus for forming and treating chlorides which comprises a closedsystem including in series a furnace, a condenser having an outletleading to a pump, a gas scrubber, and a gasreceiver, said condenserhaving an outlet into a closed tank, and a burner disposed in proximityto said closed tank.

8. Apparatus for forming and treating:

chlorides which comprises a closed system proximity to a sealed tankconnected to said condenser. I

9. In combination, a sealed furnace, a sealed condenser connectedtherewith, sealed gas receiver having sealed connection with saidcondenser, a sealed tank connected 1 with said condenser, means forheating said tank, and means for maintaining super-atmospheric pressurein said tank. I

10. In combination, a sealed furnace, a gas storage reservoir havingsealed connection therewith, said furnace having an inlet and means forsealing said inlet, and a sealed condenser connected with said fur nace,said condenser having a valved outlet.

11. In combination, a sealed furnace, a sealed condenser, and a'pump inseries are. rangement, said condenserhaving a valved outlet at thebottom thereof. y

12. In combination, a. combining chamber, a second chamber connectedtherewith, said second chamber having two portions, means formaintaining different temperatures respectively in said portions, and acollecting 15. In combination, a sealed furnace, agas storage reservoirhaving sealed'connec'tion with said furnace, said furnace having aninlet adapted to be sealed by the material fed thereto, a sealedcondenser connected with said furnace, a tank connected with saidcondenser, and a burner disposed in proximity" to said tank.

16. Apparatus for forming and treating chlorides which comprises aclosed system including a furnace, acondenscr, a pump and a gas receiverconnected in series, a sealed tank connected with an outlet from saidcondenser, and a burner disposed in proximity to said tank.

In witness whereof, I hereunto subscribe my name this first day of July,A. D. 1915.

VIOTOR'M. l/VEAVER.

